38 results about "METHOXYAMINE HYDROCHLORIDE" patented technology

The invention discloses a bufalin glycosylation derivative and a preparation method and application thereof in preparation of anti-tumour medicaments. The structure of the bufalin glycosylation derivative is shown in a formula I or formula II. The synthesis method of the bufalin glycosylation derivative comprises the following steps of: oxidizing bufalin into a ketone-form derivative by pyridinium chloropyridine hydrochloride; then performing a nucleophilic addition reaction with methoxyamine hydrochloride; removing monomolecular water to generate an oxime-form intermediate; enabling the oxime-form intermediate to react with a tert-butylamine borane hydrochloride compound to generate alpha-configuration aglycone and beta-configuration aglycone; and finally enabling the aglycones of two configurations to react with reducing sugar respectively to generate the bufalin glycosylation derivative. According to the method disclosed by the invention, bufalin is modified to be the glycosylation derivative thereof, and the water solubility can be improved while the anti-tumour activity is kept and enhanced; and moreover, in-vivo experiments prove that the toxic and side effects of the bufalin glycosylation derivative disclosed by the invention on normal cells are reduced compared with those of a parent compound of bufalin.

The invention relates to the technical field of compound synthesis methods, particularly a method for coproducing vasoxine hydrochloride and N,O-dimethylhydroxylamine hydrochloride. The method comprises the following steps: carrying out methylation reaction on hydroxylamine salt under alkaline conditions by using a methylating agent to obtain a reaction solution containing vasoxine and N,O-dimethylhydroxylamine, rectifying to separate a vasoxine bottom solution and an N,O-dimethylhydroxylamine crude distillate, respectively adding hydrochloric acid for salification, concentrating and crystallizing under reduced pressure, cooling, carrying out vacuum filtration, recrystallizing with water or methanol, and drying to obtain the vasoxine hydrochloride product and N,O-dimethylhydroxylamine hydrochloride product. The method has the advantages of simple and reliable technique, high product quality, high total yield and low comprehensive cost, and is more friendly to the environment and suitable for industrial production.

The present application discloses a method for preparing methoxyamine, which at least includes: contacting a raw material gas containing methyl nitrite and a reducing agent with a reduction reaction catalyst in a reactor to perform a reduction reaction to obtain methoxyamine. The method can fully utilize the important intermediate methyl nitrite in the coal-to-ethylene glycol process, and the conversion rate of the methyl nitrite is high. The present application also provides a preparation method of methoxyamine hydrochloride obtained by the above method as raw material.

The invention belongs to the field of synthesis of fine chemical intermediates, and discloses a method for preparing methoxyamine hydrochloride by using a microreactor. It is specifically divided into: the preparation of acetaminolamine, the preparation of acetylmethoxamine and the preparation of methoxylamine hydrochloride, wherein the preparation process of acetylhydroxylamine and acetylmethoxylamine is carried out in a microreactor. Specifically, the hydroxylamine hydrochloride solution, ethyl acetate and lye are pumped into the microchannel reaction module A, and after being mixed in the microchannel, they are pumped into the microchannel reaction module B again with dimethyl sulfate and lye, and collected after the mixed reaction. After hydrolysis, distillation, neutralization, salt formation, concentration and other processes, methoxyamine hydrochloride is obtained. Compared with the prior art, the invention effectively improves the yield of methoxyamine hydrochloride by utilizing the microreactor, reduces the generation of three wastes, shortens the reaction time and reduces the production cost.

The invention discloses a synthesis method of 4-allyl-3,5-disubstituted isoxazole, belonging to the technical field of organic synthesis. The synthesis method is as follows: in the reactor, add acetylene ketoxime ether substrate, 3-bromopropene, palladium catalyst, additive and solvent, stir and react at 70-80°C, and the reaction product is separated and purified to obtain 4-allyl -3,5-disubstituted isoxazoles. In the method of the present invention, a series of acetylenic ketone oxime ethers are obtained by reacting the product obtained through Sonogashira coupling of simple and easy-to-obtain acyl chlorides and alkynes with methoxyamine hydrochloride, the reaction conditions are mild, and there is no pollution to the environment. Potentially functional 4-allyl-3,5-disubstituted isoxazole compounds, the method is innovative and atom-economical, mild conditions, safe operation, and can be scaled up to 5 g scale without affecting the yield Therefore, it has potential practical value.

The invention provides a preparation method of a zabofloxacin intermediate. The method comprises: reacting ethyl glycinate hydrochloride with acrylonitrile under catalysis of a base to form an intermediate I; then reacting the intermediate I with Boc anhydride under the function of a strong base to generate an intermediate III; reacting the intermediate III, the methoxyamine hydrochloride and formaldehyde to generate an intermediate IV; and then preparing the zabofloxacin intermediate by reacting the intermediate IV with methanesulfonyl chloride, performing reduction with sodium borohydride, and other steps. The zabofloxacin intermediate is prepared through nine steps with a high yield and high quality by the method, the material adding amount reaches the level of hundreds of grams, and the method is suitable for industrial production.